Size for textile fabrics



Patented Apr. 18, 1944 UNITED STATES PATENT orrica SIZE FOR TEXTILE FABRICS Alfred L. Rllmmelshnrg, or to Hercules Powder Company, Wilmington, Del, a corporation Delaware I applied to improve the weaving properties.

No Drawing. Application February 14, 1942.

- Serial No. 430,884

12 Claims.

starch serves to strengthen the fibers, the gum binds the fibers together 'and the softener provides lubrication.

In the sizing of such synthetic fabrics as rayon and Nylon yarns, a sizing composition containing gelatin together with suli'onated oils or minoral oils is used.- After the weaving operation,

. 0 6 iz is generally removed from h fab i by Melting point About 50-5012; tie-sizing operation, Color il-mm 111 the 8 Of Starch sizes, con ider bl ig- 0 miiculty is encountered in removing the size from 26 pea e no 4111111 resin, V

the fab c. Starch enzymes such moval from the woven fabric. The tie-sizing of gums after weaving usually requires quite drastic treatment, such as caustic boiling under pressure. Use of sulfonated oils is not too practical because of the tendency of such materials to become rancid on ageing. Sulfonated oils also usually provide too much softening etlect and too little lubrication. Mineral oil provides certain lubricating and softening characteristics but is disadvantage that its impregnation fibers after weaving is non-uniform, usually resulting in oil spots on the fabric.

In carrying out the method in accordance with v A this invention, natural or synthetic fibers in the 50 I agi filial] I Low mu. Bi o- High Low pm. form of yarns, threads, filaments. etc are I treated with a composition containing a solution a m oil a polymerized terpene resin in mineral oil. "mm 0mm 0mm 0mm mg mg Pawn! These compositions may beapplied as an que- I 3 mac moo 137.0 2.30 am 0.60 an ous emulsion, as an organic solvent solution. as

is uneven and its removal from the i an aqueous dispersion of an organic solvent solution, or as the mineral oil solution of the polymerized terpene resin itself. The portion of polymerized terpene resin included in the mineral oil composition may be varied depending on.

the type c! sizing desired and the particular fiber being treated. Also the amount of the sizing composition employed will depend on the particular efiect desired.

To illustrate the sizing of textile fibers in aecordance with the invention, the following examples may be cited. In the examples all proportions are by welght,unless otherwise indicated.

EXAJIIPLI 1 Textile size composition containing starch modi- J fled by a polymerized t pene resin The polymerized terpene resin used in this example has the following physical properties:

St l-Emulsiflziation o] polymerized term: resin size.-A quantity of the above terpene resin was mixed with enough mineral oiltomakeabo-fiomixmre. Thismixturewm emulsified with iriethanolamine oleate.

Step 2Polym1ized terpene resin-starch szze mixture-l5 parts of the above emulsified p0 merized terpene resin ure was added to 81 i or starch and 1404 parts of water and the resulting mixture heated and agitated until the starch was thoroughly cooked.

Stcp Many of fibers-Cotton yarn we u rm: with the ve polymerized resin-starch by the it. procedure. The sized yarn showed inc w 1 tensile str and elontion over-conventional sized yarns and the ease or removability or the size from the fabric showed that it could be done with the existing Textile Exam: 2

Melting point 40-42 C. Color WW Acid number- Less than 4 Appearance Semi-hard Step I-Emulsiflcotion ol polymerized terpene resin size-A quantity the above polymerized terpene resin was mixed with enough mineral oil to make a 60-50 mixture. The mixture was emulsified with triethanolamlne oleate.

Step 2-Polumerized terpene resin-starch size mixture-25.2 parts of the polymerized terpene resinmineral oil emulsion was added to a water starch solution prepared by mixing 144 parts oi 60 fluidity corn starch and 1330 parts of water at a temperature of from '10-'15 C. with stirring. Atter the addition of the resin-mineral oil emulsion was made to the water-starch solution, the temperature of the resulting mixture was brought to about 90-95 C. at which temperature the mixture was cooked for one hour.

Step 3-Sizina of textile fibers.-The resinmineral oil emulsion-starch mixture was applied to 18/1 cotton yarn squeezed and dried. The resulting fibers showed good stiffness, smoothness. and tensile strength. The ease of removability ot this composition from the fibers was such that it would be readily removed with conventiorial equipment. The results of the tensile strength determinations made on the 18/1 cotton yarn were as follows:

A Av. break High Low Dli'i. elon- High Low Diii.

getion Per Per 0mm 0mm Gum 0mm Percent cent cent Per cent 639.6 001.0 470.0 221.0 6.18 0.70 4J0 2.00

EXAIIPLI 3 Textile size composition containing starch modifled by a polymerized terpene resin (Piccolyte 8-55) The polymerized terpene resin used in this example is known in the trade as Piccolyte 8-55 and has the following properties:

Melting point 55-58 C Color WW Acid number Less than 4 Appearance Semi-hard starch solution prepared by mixing 1440 parts 01 Gil-fluidity color starch with 1330 parts oi'water at a temperature of irom 70-75" C. with stirring. After the resin-mineral oil emulsion was added to the water-starch solution, the resulting mixture was brought to a temperature of about Gi -95 C. and the mixture cooked for one hour.

Step 3Sizina of textile jlbers.--The resinmineral oil emulsion-starch mixture was applied to 18/1 cotton yarn squeezed and dried. The resulting fibers showed good stillness, smoothness and tensile strength. The .ease of removability of this material from the fiberswas such that it would be readily removed with conventional equipment. -Results of tensile strength determinations on the 18/1 treated cotton yarn 10 are as follows:

Av. m High Imv pm. elon- High Low pm.

gation Per Per Gram 0mm Gum Gram Per cent an! cent Per cent 4216 560.0 310.0 104.0 5.43 7.1) 4.30 no i EXAIPLI 4 Polumerized terpene resin textile size composition Any one of the above resins described in the foregoing examples may be emulsified according to the following formula:

Parts Polymerized terpene resin 85 Fractol A (mineral oil) 85 Cobalt naphthenate (6%) 1 Olelc acid 19.8

8o Triethanolamine 10.2

Water 199 and used as a textile size independently oi starch or other similar material.

Step 1Emnlsiflcation operation.-The polymerized terpene resin was melted and the Fractol Step Z--Sizina of textile jlbe'rs.The resinmineral oil emulsion mixture was applied to 18/1' cotton yarn, squeezed and dried. The resulting fibers showed good stillness, smoothness and tensile strength. The ease of removabllity 0! this material'trom the fibers was such that it would be readily removed with conventional equipment.

In carrying out the method in accordance with this invention, the natural or synthetic fibers such as yarns, threads, filaments, etc., are treated with the improved polymerized terpene resin containlng size. The size may be applied as an aqueous emulsion'polymerized terpene resin in mineral oil, as an organic solvent solution of polymerized terpene resin in mineral oil, as an aqueous dispersion of an organic solvent solution 0! polymerized terpene resin modified starch emulsion.

The polymerized terpenes as, for example, the terpene polymers and copolymers which have been found to provide the desirable emulsions for textile treatment include the resinous mate rials obtained by polymerization and copolymerization of terpenes, for example, the alicyclic. monoeyciic and bicyelic terpenes and their mixtures. Specific terpenes suitable for this invention are alpha pinene, beta pinene, dlpentene, limonene, terpinene, terpinolene, allo-ocimene, myrcene. camphene, ienchene, carene, etc. in the presence of catalytic materials such as aluminum chloride, complexes of aluminum chloride with inorganic salts such as AlCia-NeCl, zinc chloride,

boron trifluoride, fullers earth. activated clay, sulfuric acid, phenol diozonium fiuoborate, phosphoric acid, tetraphosphoric acid, stannous chlo- I ride, fluoboric acid, etc.

Terpene copolymers of acyclic, monocyclic and bicyclic terpenes with other unsaturates such as styrene, coumarone, indene, cyclopentadiene, butadiene, isoprene, and isobutene are also found .suitable for the purposes of this invention.

polymers. of terpenes with halogenated unsatuoperable.

Hydrogenated products of each of these terpene polymers and copolymers are found desirable for the purposes of this invention.

The polymerized terpenes which are effective rates as, for example, vinyl chloride-are found in providing the improvements in accordance with this invention are those which are either viscose liquids at ordinary temperatures or soft solids melting up to about 150 C. by the drop method. Preferably, the polymerized terpenes melting at about 40 C. to about 80 C. will be used.

Terpene polymers as, for example, the "Piccolyte resins herein disclosed may be prepared by procedures well known in the art. The polymerized terpene resin disclosed in Example 1 may be prepared as follows:

To 188 g. of anhydrous aluminum chloride, add 1250 g. of ethylenedichloride. Cool the mixture to 34 F. and add 750 g. of alpha-pinene during 2% hours with vigorous agitation, maintaining the temperature at about 65 to 70 F.. remove the cooling and agitate the homogeneous solution for hour at 60- to 70 F. Cool the solution to 40 F. and add 100 g. of ice with stirring during about 10 minutes, during which time the tern perature will increase to about 120 F. Add to this mixture about 500 cc. of water with agitation for 15 minutes, thoroughly wash the ethylene dichloride solution and remove the ethylene dichloride by steam distillation. The yield will be about 650 g. of resin. The product is then heated to about 260 F. for about y hour under a blanket of carbon dioxide as a means of bleaching the color. The physical characteristics of this resin will be as follows:

Melting point 50-60 C. Colon- About '30 amber Odor Balsam-like )Appearance. Semi-hard resin formu1ations. Mineral oil solutions of the p01?- merized terpenesmay be used in the range of about 10 to 85% of polymerized terpene, but preferably in the range of about 40 to 70% of the polymerized terpene. a

. In the preparation of emulsions of the polymerized terpene resin with mineral oil, the following emulsifying agents may be used as, for example, the alkali metal salts of the higher aliphatic ester sulfates, as sodium lauryl sulfate.

sodium stearyl sulfate, sulfonated oils as sulfonated castor oil, sulfonated olive oil, soaps as sodium stearate, sodium oleate, potassium ole'ate, alkali metal salts and alkali naphthenic sulfuric acids as sodium butyl naphthenatesulfonate,sodium isopropy1- naphthenate' sulfonate, triethanolamine, etc. 1

It is found that yarn sized with sizing compositions containing the above polymerized terpene resin-mineral oil solutions or emulsions of this solution have the following advantages over the conventional prior art starch sized yarns in that the polymerized resin sized yarn has a greater tensile strength, has less solids deposited on the yarn, has a greater smoothness and pliability characteristic, and has a greater effect on decreasing the amount of yarn shredding during weaving operations.

What I claim and desire to protect by Letters Patent is:

1. A textile fiber size comprising a mineral oil aqueous emulsion of a polymerized terpene hydrocarbon resin. 2. A textile fiber size comprising a mineral oil aqueous emulsion of a polymerized terpene hydrocarbon resin, the resin being characterized as having a melting point between about 40 C. and

about 80 C.

s. A textile fiber size comprising a mineral oil pene hydrocarbon resin-, the resin being characterized as having a melting point up to about C. j

6. A. textile fiber starch size comprising a mineral oil aqueous emulsion of a polymerized terpene hydrocarbon resin, the resin being characterized as having a melting point between about 40? C; and about 42 C.

'7. A textile flber starch size comprising a mineral oil aqueous emulsion of a polymerized terpene hydrocarbon resin, the resin being characterized as having a melting point between about 55 C. and 58 C.

8. The method of sizing textile fibers prior to weaving which comprises treating the fibers with a composition comprising a solution of a polymerized terpene hydrocarbon resin in mineral oil.

9. The method of sizing textile fibers prior to weaving which comprises treating the fibers with a. composition comprising a solution of between about 10% to about 85% of polymerized hydrocarbon resin and mineral oil.

10. The method of sizing textile fibers prior to weaving which comprises treating the fibers with a composition comprising a solution of between about 40% to about of polymerized terpene hydrocarbon resin in mineral oil. 11. Atextile fiber sized with a composition comprising a'mineral oil aqueous emulsion of a polymerized-terpene hydrocarbon resin, the resin being characterized by havinga melting point between about 40 C. and about 60 C.

12. A textile fiber sized witha composition comprising a mineral oil aqueous emulsion of a polymerized terpene hydrocarbon resin, the resin being characterized by having a melting point between about 40 C; and about C.

' ALFRED L RUMMELSBURG.

terpene 

